CN104759265B - A kind of preparation method of porous foams heavy-metal adsorption material - Google Patents
A kind of preparation method of porous foams heavy-metal adsorption material Download PDFInfo
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Abstract
The invention provides a kind of method that hole foams heavy-metal adsorption material is prepared utilization High Internal Phase Emulsion template, belonging to technical field of polymer materials more.This method is using water as continuous phase, organic solvent is discontinuous organic phase, nonionic surfactant is emulsion stabilizer, chitosan is used as grafting skeleton, polymerizable function monomer is grafted monomers, in the presence of initiator, crosslinking agent, it is white porosity foam-body material that form, which is made, by High Internal Phase Emulsion template.Experiment shows, porous adsorbing material prepared by the present invention is not only containing abundant pore passage structure, it is greatly improved the rate of adsorption and adsorption capacity of heavy metal, and with extraordinary reusable performance, product form is porous foams simultaneously, and being administered for heavy-metal contaminated soil has the advantages that easy to use and recoverable.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of preparation method of heavy-metal adsorption material, especially
It is related to a kind of method that hole foams heavy-metal adsorption material is prepared utilization High Internal Phase Emulsion template more.
Background technology
Heavy metal is present among the environment such as water body, soil and air with a variety of physics and chemical form, and in the environment
Produce migration, enrichment, absorb and conversion, so that be detrimental to health by food chain, such as carcinogenic, teratogenesis.With China's work
The development of industry, current water body and heavy metal pollution of soil turn into the difficult point administered.
Environmental Protection Department and Ministry of Land and Resources's issue《National Soil Pollution Investigation publication》Point out, national soil is total
Exceeding standard rate is 16.1%, and cadmium, lead point position exceeding standard rate respectively reach 7.0% and 1.5% wherein in soil.How safely and effectively to repair
And turned into the environment and social concern of current China's urgent need to resolve using these contaminated heavy metal soil.Using adsorption material
Material is removed or in-situ passivation heavy metal in soil is because with investing, small, method is simple, the more low advantage of cost, in a huge sum of money
There is great application prospect in category pollution control field.
In-situ passivation Principles are by adding organic and inorganic or hydridization functional material etc. into contaminated soil, to adjust
Section and change soil physico-chemical property, it is produced absorption, precipitation, ion exchange, oxidationreduction etc. and react, change heavy metal from
Chemical form and occurrence status of the son in soil, suppress its transportable property and biological effectiveness in soil, reduce crops
The uptake and accumulation of heavy metal, and then reach the purpose of repairing polluted soil.But in-situ passivation recovery technique is to cure the symptoms, not the disease
Method, thus it is real economical, effectively, the heavy metal-polluted soil that can use on a large scale removes recovery technique turns into the mesh that people pursue
Mark.
Removing heavy metals are removed from contaminated soil, one is the optional adsorptivity of sorbing material to be solved, and two be to solve
Material is from the separability in soil.Made important progress in recent years in terms of adsorptivity may be selected in heavy metal, but adsorption material
How material separates aspect in soil with soil work after Adsorption of Heavy Metals is seldom.Current sorbing material is generally powdered products
It is difficult that can be efficiently separated from soil after product, with soil blending absorption.Therefore, develop the recyclable of function admirable or be easy to soil
The adsorbent of separation, as the emphasis for administering heavy metal pollution of soil concern.
In recent years, people gradually recognize that large pore material has quick adsorption and desorption feature in adsorption separation process,
Not only adsorption efficiency is high and recoverable, while by hole wall modification material can be made to have good Selective adsorption, therefore
There is easy to use, recoverable in terms of heavy-metal contaminated soil improvement.
The content of the invention
It is an object of the invention to provide one kind porous foams heavy metal adsorption material is prepared using High Internal Phase Emulsion template
The method of material.
First, the preparation of porous foams heavy-metal adsorption material
The preparation of porous foams heavy-metal adsorption material of the present invention, is that, using water as continuous phase, organic solvent is organic point
Dephasing, nonionic surfactant is emulsion stabilizer, and chitosan is as grafting skeleton, and polymerizable function monomer is single for grafting
Body, in the presence of initiator, crosslinking agent, is prepared by High Internal Phase Emulsion template.
Its specific preparation technology is：First chitosan, polymerizable function monomer, crosslinking agent, initiator are filled under agitation
It is dispersed in water, then stirs fully dispersed adding discontinuous organic phase into aqueous phase, obtains high concentrated emulsions；It is then charged into stylostome
In in 30 ~ 90 DEG C polymerize 4 ~ 48h after, 12 ~ 48h of surname extraction is dehydrated through industrial alcohol, and vacuum does drying, obtains porous foam
Body weight metal-adsorbing material.
In above-mentioned reaction medium, continuous phase water is matched with discontinuous organic phase by volumes below percentage：Water 10% ~
40%, discontinuous organic phase 60% ~ 90%.
Above-mentioned each raw material is matched by following mass percent：Surfactant 10% ~ 50%, chitosan 5 ~ 20%, can
The function monomer 10 ~ 40% of polymerization, crosslinking agent 1 ~ 25%, initiator 0.2 ~ 10%.
Wherein, it is toluene, benzene, paraxylene, atoleine, n-hexane, positive heptan as the organic solvent of discontinuous organic phase
One kind in alkane, normal octane, n-decane, turpentine oil, carbon tetrachloride.
Surfactant is AEO, alkylphenol polyethylene oxide ether, fatty acid polyglycol cyclic ethylene alkyl ester, poly-
Oxireme alkylamine, polyxyethylated acyl hydramine, polyoxyethylene and polyoxypropylene block copolymers, fatty acid glyceride,
At least one of sucrose fatty ester, Span and sorbitan fatty acid ester.
Polymerizable function monomer be acrylamide,N- N-isopropylacrylamide, maleic acid, acrylic acid, methacrylic acid,
Methyl methacrylate, hydroxyethyl methacrylate, hydroxy propyl methacrylate, butyl acrylate, styrene, 2- acryloyls
Amine -2- methyl-propanesulfonic acids, itaconic acid, vinylpyrrolidone, acrylamide -4- vinyl pyrimidines, vinyl imidazole, pi-allyl
At least one of imidazoles.
Crosslinking agent is ethylene glycol dimethacrylate, trimethylolpropane trimethacrylate, trimethylolpropane tris first
Base acrylate, triallyl isocyanate,N,N’One kind in-methylene-bisacrylamide.
Initiator is one kind in potassium peroxydisulfate, ammonium persulfate, azodiisobutyronitrile, benzoyl peroxide.
2nd, the structure of porous foams heavy-metal adsorption material, morphology characterization
It is right below by the characterization method such as laser scanning co-focusing microscope (CLSM) and SEM (SEM)
High Internal Phase Emulsion and the structure and morphology of porous heavy metal absorbent prepared by the present invention is analyzed.
1st, laser scanning co-focusing microscope (CLSM) is analyzed
The pattern for the High Internal Phase Emulsion that Fig. 1 is prepared for the present invention.In emulsion preparation process, respectively in dispersed phase and continuously
Fluorescent color-developing agent perylene and fluorescein are added in phase, then High Internal Phase Emulsion is entered under laser scanning co-focusing microscope
Row observation.In light bright spot it is that continuous part is water continuous phase in discontinuous organic phase, b in a in figure.It can be seen that
Discontinuous organic phase is uniformly distributed and close-packed arrays in High Internal Phase Emulsion, part discontinuous organic phase in regular circle shapes and part then
Irregular polygon is presented, because during large percentage shared by disperse phase volume, a large amount of organic solvent liquids are crowded together
Formed.Moreover, moisture dephasing is extruded into thin layer in emulsion by organic continuous phases, but still it is continuously distributed.These message certifications,
By this kind of High Internal Phase Emulsion preparation method, oil-in-water type High Internal Phase Emulsion is ultimately formed（O/W）.
2nd, sem analysis
Digital photograph and the SEM figure for the porous adsorbent that Fig. 2 is prepared for the present invention.From digital photograph as can be seen that originally
The product form for inventing the porous adsorbing material prepared is white porosity foams, diameter of section about 0.5cm.Can be with from SEM figures
It was observed that porous adsorbent has a large amount of pore passage structures, wherein one-level hole aperture is in 0.5 ~ 5um, and second hole largely exists and is distributed
Uniformly.One-level hole and second hole it is a large amount of be distributed with beneficial to heavy metal ion from extraneous solution to sorbing material diffusion inside,
It is final to realize the quick of heavy metal, efficient absorption separation.
3rd, the absorption of porous foams heavy-metal adsorption material heavy metal and repeat performance
1st, the absorption property of heavy metal lead and copper
50mg/L, 200mg/L and 500 mg/L Pb are chosen respectively2+And Cu2+Simulate heavy metal wastewater thereby 25 mL, Xiang Qi
It is middle to add adsorbent of the present invention（Initial amount is 0.8 g/L）, constant temperature oscillation difference adsorption time is separated by filtration, supernatant is with can
See spectrophotometry Pb2+And Cu2+Concentration.Fig. 3, Fig. 4 are respectively the porous adsorbent of the invention prepared to Cu2+, Pb2+
Adsorpting rate curve.From Fig. 3,4, either Pb2+Or Cu2+, in 50mg/L, its time of equilibrium adsorption is 5min；
In 500mg/L, its time of equilibrium adsorption is 20min, and the result illustrates either low concentration or high concentration heavy metal ion,
It can realize that quick adsorption is removed, its adsorption capacity is to Pb2+Maximum reachable 605 mg/g, to Cu2+Maximum reachable 332mg/L.
2nd, the repeat performance of heavy metal lead and copper
Choose 500 mg/L Pb2+And Cu2+Heavy metal wastewater thereby 25mL is simulated, adsorbent of the present invention is added thereto（Starting
Measure 0.8g/L）, constant temperature oscillation 1h is separated by filtration.Supernatant determines Pb with visible spectrophotometry2+And Cu2+Concentration.Absorption
After agent filtering, continue on for after 0.1mol/L HCl solutions desorption, the regeneration of 0.1mol/L NaOH solutions to Pb2+And Cu2+Simulation
Heavy metal wastewater thereby is adsorbed.Fig. 5,6 are respectively the porous adsorbent Adsorption of Cu of the invention prepared2+, Pb2+Repeat performance it is bent
Line.As seen from the figure, either for Pb2+Or Cu2+, porous adsorbent after 5 adsorption-desorption processes, remain in that very well
Absorption property, adsorption capacity reduction be respectively less than 5%.Illustrate that this kind of porous heavy metal absorbent has fine repeat performance.
In summary, the present invention has advantages below compared with the prior art：
1st, using High Internal Phase Emulsion technology, stable oil-in-water type can be formed（O/W）After High Internal Phase Emulsion, thus polymerization
There is substantial amounts of one-level hole and second hole, it is possible to achieve heavy metal Cu2+And Pb2+Rapidly and efficiently absorption；
2nd, adsorbent prepared by the present invention has extraordinary reusable performance, effectively reduces heavy metal polluted soil
The cost that earth is administered；
3rd, adsorbent product form prepared by the present invention is porous foams, and administering to have for heavy-metal contaminated soil makes
The advantages of with convenient and recoverable.
Brief description of the drawings.
Laser scanning co-focusing microscope (CLSM) figure for the high concentrated emulsions that Fig. 1 is prepared for the present invention.
Outward appearance photo and the SEM figure for the porous heavy metal absorbent that Fig. 2 is prepared for the present invention.
Fig. 3 is the porous adsorbent of the invention prepared to Cu2+Adsorpting rate curve.
Fig. 4 is the porous adsorbent of the invention prepared to Pb2+Adsorpting rate curve.
The porous adsorbent Adsorption of Cu that Fig. 5 is prepared for the present invention2+Repeat performance curve.
The porous adsorbent absorption Pb that Fig. 6 is prepared for the present invention2+Repeat performance curve.
Embodiment
Preparation and its absorption property with reference to embodiment to adsorbent of the present invention are described in detail.
Embodiment 1
By 0.5g chitosans, 2.0g acrylamides, 2.0g acrylic acid, 1.25g under 500rpm stirringsN,N’- methylene
Bisacrylamide, 3.5g fatty alcohol polyethenoxy ether class surfactant, initiator potassium persulfate 0.5g are scattered in 10 mL water
In；Treat after each component dissolving, atoleine 60mL stirrings 4h is added into mixed liquor；The high concentrated emulsions of gained load stylostome,
Sealing, polymerize 12h in 50 DEG C.Resulting polymers n-hexane surname extraction 48h, after industrial alcohol dewater treatment, vacuum drying,
Obtain porous adsorbing material.Sorbing material heavy metal Cu2+And Pb2+Go adsorbance to be respectively 325 mg/g and 586mg/
g。
Embodiment 2
By 1.0g chitosans, 2.0g 2- acrylamide -2- methyl-propanesulfonic acids, 1.0g metering systems under 300rpm stirrings
Sour methyl esters, 0.5 g ethylene glycol dimethacrylates, 2.0g Span class surfactants and 2.0g polyoxyethylene
It is scattered in polyoxypropylene block copolymers class surfactant, initiator ammonium persulfate 0.2g in 20 mL water；Treat each component
After dissolving, normal octane 60mL stirrings 1h is added dropwise into mixed liquor；The high concentrated emulsions of gained load stylostome, sealing, in 40 DEG C
It polymerize 24h.Resulting polymers n-hexane surname extraction 12h, after industrial alcohol dewater treatment, vacuum drying obtains porous suction
Enclosure material.Sorbing material heavy metal Cu2+And Pb2+Go adsorbance to be respectively 218 mg/g and 524mg/g.
Embodiment 3
By 1.0 g chitosans, 2.0g methacrylic acids and 0.5 g hydroxy propyl methacrylates, 2.5 under 600rpm stirrings
G trimethylol-propane trimethacrylates, 5.0g alkylphenol polyethylene oxides ether surfactant, initiator ammonium persulfate
0.75g is scattered in 15 mL water；Treat after each component dissolving, toluene 55mL stirrings 1h is added dropwise into mixed liquor；Gained is high
Concentrated emulsions load stylostome, and sealing polymerize 12h in 50 DEG C.Resulting polymers n-hexane surname extraction 24h, it is de- through industrial alcohol
After water process, vacuum drying obtains porous adsorbing material.Sorbing material heavy metal Cu2+And Pb2+Go adsorbance to distinguish
For 332 mg/g and 605mg/g.
Embodiment 4
By 2.0 g chitosans, 2.0g itaconic acids, 2.0g 2- acrylamide -2- methyl-propanesulfonic acids under 600rpm stirrings
And 0.2gN,N’- methylene-bisacrylamide, 4.0g fatty alcohol polyethenoxy ether class surfactant, initiator potassium persulfate
0.5g is scattered in 5 mL water；Treat after each component dissolving, carbon tetrachloride 35mL stirrings 1h is added dropwise into mixed liquor；Gained
High concentrated emulsions load stylostome, and sealing polymerize 12h in 80 DEG C.Resulting polymers n-hexane surname extraction 48h, through industrial alcohol
After dewater treatment, vacuum drying obtains porous adsorbing material.Sorbing material heavy metal Cu2+And Pb2+Go adsorbance point
Wei not 288 mg/g and 517mg/g.
Embodiment 5
By 0.75 g chitosans, 2.0g under 300rpm stirrings N- N-isopropylacrylamide, 1.0g allyl imidazoles and
0.2g N,N’- methylene-bisacrylamide, 4.0g polyoxyethylene and polyoxypropylene block copolymers class surfactant, initiation
Agent ammonium persulfate 0.5g is scattered in 10 mL water；Treat after each component dissolving, paraxylene 45mL is added dropwise into mixed liquor
Dispersed with stirring 1h；The high concentrated emulsions of gained load test tube, and sealing polymerize 24h in 50 DEG C.Resulting polymers n-hexane surname extraction
24h, after industrial alcohol dewater treatment, vacuum drying obtains porous adsorbing material.Sorbing material heavy metal Cu2+And Pb2 +Go adsorbance to be respectively 263 mg/g and 476mg/g.
Claims (6)
1. a kind of preparation method of porous foams heavy-metal adsorption material, is that, using water as continuous phase, organic solvent is organic point
Dephasing, nonionic surfactant is emulsion stabilizer, and chitosan is as grafting skeleton, and polymerizable function monomer is single for grafting
Body, in the presence of initiator, crosslinking agent, is prepared by High Internal Phase Emulsion template；Specifically preparation technology is：Stirring is lower first
Chitosan, polymerizable function monomer, nonionic surfactant, crosslinking agent, initiator are well-dispersed in water, then to water
Discontinuous organic phase stirring is added in phase fully dispersed, obtain high concentrated emulsions；It is then charged into stylostome, polymerize 4 ~ 48h in 30 ~ 90 DEG C
Afterwards, 12 ~ 48h of surname extraction, is dehydrated through industrial alcohol, and vacuum does drying, obtains porous foams heavy-metal adsorption material；
The polymerizable function monomer be acrylamide,N- N-isopropylacrylamide, maleic acid, acrylic acid, methacrylic acid,
Methyl methacrylate, hydroxyethyl methacrylate, hydroxy propyl methacrylate, butyl acrylate, styrene, 2- acryloyls
Amine -2- methyl-propanesulfonic acids, itaconic acid, vinylpyrrolidone, acrylamide -4- vinyl pyrimidines, vinyl imidazole, pi-allyl
At least one of imidazoles；
The nonionic surfactant is AEO, alkylphenol polyethylene oxide ether, fatty acid polyglycol cyclic ethylene
Alkyl ester, Pluronic F-127 alkylamine, polyxyethylated acyl hydramine, polyoxyethylene and polyoxypropylene block copolymers, glyceride
At least one of fat acid esters, sucrose fatty ester, Span and sorbitan fatty acid ester；
Each raw material is matched by following mass percent：Nonionic surfactant 10% ~ 50%, chitosan 5 ~ 20%,
Polymerizable function monomer 10 ~ 40%, crosslinking agent 1 ~ 25%, initiator 0.2 ~ 10%.
2. the preparation method of porous foams heavy-metal adsorption material as claimed in claim 1, it is characterised in that：Continuous phase water with
Discontinuous organic phase is matched by volumes below percentage：Water 10% ~ 40%, discontinuous organic phase 60% ~ 90%.
3. the preparation method of porous foams heavy-metal adsorption material as claimed in claim 1, it is characterised in that：Described organic point
Dephasing is in toluene, benzene, paraxylene, atoleine, n-hexane, normal heptane, normal octane, n-decane, turpentine oil, carbon tetrachloride
One kind.
4. the preparation method of porous foams heavy-metal adsorption material as claimed in claim 1, it is characterised in that：The crosslinking agent
For ethylene glycol dimethacrylate, trimethylolpropane trimethacrylate, trimethylol-propane trimethacrylate, triolefin
Propylisocyanate,N,N’One kind in-methylene-bisacrylamide.
5. the preparation method of porous foams heavy-metal adsorption material as claimed in claim 1, it is characterised in that：The initiator
For one kind in potassium peroxydisulfate, ammonium persulfate, azodiisobutyronitrile, benzoyl peroxide.
6. the preparation method of porous foams heavy-metal adsorption material as claimed in claim 1, it is characterised in that：Mixing speed is
300~600rpm。
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| CN105289557A (en) * | 2015-10-15 | 2016-02-03 | 中国科学院兰州化学物理研究所 | Method for preparing magnetic aerogel adsorption material by using Pickering-high-internal-phase emulsion template method |
| CN105664897A (en) * | 2016-02-29 | 2016-06-15 | 中国科学院兰州化学物理研究所 | Method for preparing magnetic porous microsphere adsorbing material by utilizing O/W/O double emulsion template |
| CN106902875B (en) * | 2017-02-24 | 2019-03-01 | 同济大学 | A method of utilizing the porous catalyst material of High Internal Phase Emulsion template method preparation surface gold nanoparticle modification |
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| CN107442081B (en) * | 2017-08-18 | 2021-03-26 | 中国科学院兰州化学物理研究所 | Method for constructing porous heavy metal adsorbent by taking Pickering water-based foam as template |
| CN109482158B (en) * | 2018-11-28 | 2021-08-27 | 中国科学院兰州化学物理研究所 | Method for preparing high-performance three-dimensional network adsorbent by semi-dry method |
| CN109967044A (en) * | 2019-04-08 | 2019-07-05 | 青岛农业大学 | The chitosan multi-porous gel rubber material and preparation method thereof that in Pickering- high prepared by phase solution template |
| CN110479756B (en) * | 2019-08-23 | 2021-11-30 | 长沙凯泽工程设计有限公司 | Soil remediation process |
| CN111229177A (en) * | 2020-02-11 | 2020-06-05 | 南通大学 | Poly- (styrene-divinylbenzene-vinyl imidazole) @ Fe3O4Water treatment agent and preparation method thereof |
| CN111185478A (en) * | 2020-03-13 | 2020-05-22 | 昆明理工大学 | Method for restoring cadmium-polluted soil based on switch surfactant |
| CN111632563A (en) * | 2020-05-21 | 2020-09-08 | 扬州大学 | Hydrogel microsphere based on microfluidic technology and preparation method thereof |
| CN112872003A (en) * | 2021-04-15 | 2021-06-01 | 四川农业大学 | Method for leaching and repairing copper in mine polluted soil |
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| US5985434A (en) * | 1997-11-25 | 1999-11-16 | Kimberly-Clark Worldwide, Inc. | Absorbent foam |
| JP4749531B2 (en) * | 2000-07-05 | 2011-08-17 | 株式会社日本触媒 | Method for producing porous polymer |
| JP2004514006A (en) * | 2000-11-07 | 2004-05-13 | ザ、プロクター、エンド、ギャンブル、カンパニー | Fiber reinforced foam composites obtained from high internal phase emulsions |
| CN100562530C (en) * | 2005-07-27 | 2009-11-25 | 中国科学院过程工程研究所 | Preparation method of a kind of super large pore polymer microsphere and products thereof |
| CN101735389B (en) * | 2009-12-17 | 2012-02-08 | 华东理工大学 | Emulsion template method for preparing soap free hydrophilic polymer porous material |
| CN102675540B (en) * | 2011-03-15 | 2014-11-26 | 中南林业科技大学 | Heavy metal ion adsorption resin and preparation method thereof |
| CN103894395B (en) * | 2014-03-24 | 2016-04-13 | 华南理工大学 | A kind of method that heavy-metal contaminated soil secondary is repaired |
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